Reactive distillation-vapor permeation coupling process for polyoxymethylene dimethyl ether synthesis

A technology of polyoxymethylene dimethyl ether and reactive distillation, which is applied in the preparation of organic compounds, chemical industry, sustainable manufacturing/processing, etc., and can solve problems such as complex product components, complicated separation process, and high energy consumption

Active Publication Date: 2019-08-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods all have anhydrous chain growth reactant (as, paraformaldehyde, gas-phase formaldehyde, paraformaldehyde) reaction raw material price is higher, product economy is not high, lacks market competitiveness
Patent CN108383696A proposes a method for preparing polyoxymethylene dimethyl ether by reacting aqueous paraformaldehyde and methylal, but the preparation of polyoxymethylene dimethyl ether in this method uses a reactor, and the product components after the reaction are complex and There is still a small amount of water, the subsequent separation is more difficult, and the energy consumption required to obtain DMM3~5 in the proces

Method used

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  • Reactive distillation-vapor permeation coupling process for polyoxymethylene dimethyl ether synthesis
  • Reactive distillation-vapor permeation coupling process for polyoxymethylene dimethyl ether synthesis
  • Reactive distillation-vapor permeation coupling process for polyoxymethylene dimethyl ether synthesis

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Embodiment 1

[0060] The method of the present invention is used for the polyoxymethylene dimethyl ether process of methylal and water-containing paraformaldehyde reaction under acidic conditions, and methylal and water-containing paraformaldehyde are obtained from the polyoxymethylene dimethyl ether reaction rectification tower respectively The two liquid-phase feed ports on the reaction section enter into the polyoxymethylene dimethyl ether reactive distillation column, and the methylal feed port is below the water-containing paraformaldehyde feed port. The mass ratio of formaldehyde to methylal in the raw material paraformaldehyde of the polyoxymethylene dimethyl ether reactive distillation column is 3, the working pressure of the polyoxymethylene dimethyl ether reactive distillation column is an absolute pressure of 6 atm, and the catalyst adopts Acidic resin, catalyst consumption is 200kg / m 3 , The height of the catalytic packing in the reaction section is 2.5 meters, the height of the...

Embodiment 2

[0063] The method of the present invention is used for the reaction system polyoxymethylene dimethyl ether process of methylal and water-containing paraformaldehyde under acidic conditions, and methylal and water-containing paraformaldehyde are obtained from the polyoxymethylene dimethyl ether reaction rectification tower respectively The two liquid-phase feed ports on the reaction section enter into the polyoxymethylene dimethyl ether reactive distillation column, and the methylal feed port is below the water-containing paraformaldehyde feed port. The mass ratio of formaldehyde to methylal in the raw material paraformaldehyde of the polyoxymethylene dimethyl ether reactive distillation column is 4.5, the working pressure of the polyoxymethylene dimethyl ether reactive distillation column is 7 atm absolute pressure, and the catalyst adopts Acidic molecular sieve, catalyst consumption is 100kg / m 3 , There are 15 catalytic trays in the reaction section, 25 trays in the rectifica...

Embodiment 3

[0066] The method of the invention is used in the process of preparing polyoxymethylene dimethyl ether by reacting methylal and water-containing gas-phase formaldehyde under acidic conditions. Methylal and water-containing gas-phase formaldehyde enter the polyoxymethylene dimethyl ether reactive distillation tower from the liquid-phase feed port and the gas-phase feed port on the polyoxymethylene dimethyl ether reactive distillation tower respectively, and formaldehyde The aldehyde feed port is above the water-containing vapor phase formaldehyde feed port. The mass ratio of formaldehyde to methylal in the raw material gas phase formaldehyde of the polyoxymethylene dimethyl ether reactive distillation column is 0.6, the working pressure of the polyoxymethylene dimethyl ether reactive distillation column is an absolute pressure of 2 atm, and the catalyst adopts acidic Resin, catalyst consumption is 300kg / m 3 The height of the catalytic packing in the reaction section is 4 meter...

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Abstract

The invention relates to a reactive distillation-vapor permeation coupling process for the polyoxymethylene dimethyl ether synthesis. According to the coupling process, a methylal and a formaldehyde solution, a hydrous trioxymethylene, a hydrous paraformaldehyde, a hydrous gaseous formaldehyde or a mixture of substances are used as raw materials, a polyoxymethylene dimethyl ether mixed product with multiple polymerization degrees is obtained by carrying out a reaction under the action of an acidic catalyst, by the separation action of a polyoxymethylene dimethyl ether reactive distillation tower, reaction products with polymerization degrees of more than 2 are extracted out from the tower kettle, DMM2 with low polymerization degrees, unreacted methylal, reaction by-product methanol, and water in the reaction system are extracted out from the tower top, the extracted products from the tower kettle is subjected to product refining tower separation, and the target product DMM3-5 is obtained. According to the process, defects in the existing process that the target product DMM3-5 has low yield, the circulation amount in the process is large, the energy consumption is high, and the likeare solved, the reaction balance limit can be broken, the conversion rate of the raw material and the selectivity and yield of DMM3-5 are greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemical production technology and equipment, and relates to the synthesis and separation and purification of polyoxymethylene dimethyl ether, in particular to a reactive distillation-steam permeation coupling process device for synthesizing polyoxymethylene dimethyl ether and method. Background technique [0002] With the increase of diesel demand, the exhaust emission problem is becoming more and more serious. Diesel combustion performance can be improved by adding appropriate additives, which will bring economic and environmental benefits. According to the use characteristics of compression ignition of diesel engines and the characteristics of oxygen-containing fuels, oxygen-containing compounds can reduce the soot and soot during diesel combustion, and are suitable as diesel additives. Polyoxymethylene dimethyl ether has a relatively high oxygen content and cetyl octane number. Adding an appropriate...

Claims

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Application Information

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IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCC07C41/56C07C41/58C07C43/30Y02P20/10
Inventor 高鑫孟莹李洪韩振为从海峰李鑫钢
Owner TIANJIN UNIV
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